Audio products

Abstract

The present invention provides an adhesive composition that is particularly suitable for bonding facings to acoustic elements, uses renewable raw materials as starting materials, reduces or eliminates corrosive and / or harmful materials, and is relatively inexpensive to manufacture, and an acoustic product formed from the acoustic element bonded to the facing. [Solution] The adhesive is a phenol- and formaldehyde-free aqueous adhesive composition, comprising component (i) in the form of one or more lignosulfonate lignins having a carboxylic acid group content of 0.03 to 2.0 mmol / g, for example, 0.03 to 1.4 mmol / g, for example, 0.075 to 2.0 mmol / g, for example, 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin, and component (ii) in the form of one or more crosslinkers.

Description

[Technical Field]

[0001] The present invention relates to acoustic products for sound insulation and absorption, and in particular to methods of making such products and systems including such products. [Background technology]

[0002] It is well known to provide acoustical products for sound absorption and insulation. A common form of such product is a panel-like acoustic element having a facing adhered to a major surface of the panel.

[0003] It is important that the adhesive used to bond the facing to the panel has suitable properties, particularly adequate bond strength (usually defined in terms of peel strength).

[0004] It is common to use phenol-formaldehyde resins as adhesives for facings. This is particularly useful in connection with acoustical panels formed from a matrix of man-made vitreous fiber (MMVF) bonded by a binder, because phenol-formaldehyde resins are already commonly used as binders for such products. Phenol-formaldehyde adhesives provide good results and are commonly used commercially.

[0005] Phenol-formaldehyde resins can be produced economically and can be mixed with urea prior to use as binders. However, current laws and legislation aimed at reducing or eliminating formaldehyde emissions have led to the development of formaldehyde-free binders, such as binder compositions based on polycarboxy polymers and polyols or polyamines, as disclosed, for example, in EP-A-583086, EP-A-990727, EP-A-1741726, US-A-5,318,990, and US-A-2007 / 0173588.

[0006] Another group of non-phenol-formaldehyde binders are addition / elimination reaction products of aliphatic and / or aromatic anhydrides with alkanolamines, as disclosed, for example, in WO 99 / 36368, WO 01 / 05725, WO 01 / 96460, WO 02 / 06178, WO 2004 / 007615, and WO 2006 / 061249. These binder compositions are water-soluble and exhibit excellent binding properties in terms of cure speed and cure density.

[0007] WO2008 / 023032 discloses urea modified binders of a type that provide mineral wool products with reduced moisture absorption.

[0008] These could in principle be used as adhesives for facings in acoustic elements, but since some of the starting materials used in the production of these binders are rather expensive chemicals, there is currently a need to provide economically produced formaldehyde-free adhesives.

[0009] A further consequence associated with previously known aqueous adhesive compositions for mineral fibers is that at least a large proportion of the starting materials used in the production of these binders are derived from fossil fuels. Current consumer trends favor products that are made entirely or at least partially from renewable raw materials, and therefore there is a need to provide binders for mineral wool that are made at least partially from renewable raw materials.

[0010] A further drawback associated with previously known aqueous adhesive compositions for mineral fibers is that they contain corrosive and / or harmful components. This requires protective measures for the machinery involved in the production of mineral wool products to prevent corrosion, and also requires safety measures for the personnel who operate the machinery. This leads to increased costs and health problems, and therefore there is a need to provide adhesive compositions with a reduced content of corrosive and / or harmful materials.

[0011] On the other hand, numerous binders for mineral fibers are available that are based largely on renewable starting materials, and in many cases, these binders that are based largely on renewable resources are also formaldehyde-free.

[0012] However, many of these binders are still relatively expensive because they are based on relatively expensive basic materials that make them uneconomical to use as adhesives to bond facings to acoustic elements. Summary of the Invention [Problem to be solved by the invention]

[0013] It is therefore an object of the present invention to provide an adhesive composition that is particularly suitable for bonding facings to acoustic elements, that uses renewable raw materials as starting materials, that reduces or eliminates corrosive and / or harmful materials, and that is relatively inexpensive to manufacture.

[0014] It is a further object of the present invention to provide an acoustical product formed from an acoustical element bonded to a facing, which has good adhesive properties, particularly those provided by phenol-formaldehyde binders, but which minimizes the disadvantages of phenol-formaldehyde binders. [Means for solving the problem]

[0015] According to a first aspect of the present invention, we have provided a method of manufacturing an acoustic product, comprising: providing an acoustic element including first and second major surfaces; providing a first facing; securing a first facing to the first major surface of the acoustic element with an adhesive; and The process of curing the adhesive wherein the adhesive is a phenol- and formaldehyde-free aqueous composition; and component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (ii) in the form of one or more crosslinkers The method includes:

[0016] In the present invention, we use an adhesive composition as defined above, which has the advantage of providing adhesive properties that are commercially acceptable and practically comparable to those of phenol-formaldehyde resins, but without the attendant drawbacks.

[0017] According to a second aspect of the invention, we provide an acoustic product obtainable by the method of the first aspect of the invention.

[0018] According to a third aspect of the present invention, we provide an acoustic product comprising an acoustic element including first and second major surfaces and a first facing, the first facing being in contact with the first major surface of the acoustic element. and the adhesive before hardening is an aqueous adhesive composition that does not contain phenol or formaldehyde; component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (ii) in the form of one or more crosslinkers The present invention provides the above product, which includes:

[0019] A preferred method of making an acoustic product includes applying a second facing to a second major surface of the acoustic element before curing, and, after curing, cutting the acoustic element into two equal halves parallel to the major surfaces. Each half has a cut surface that defines the front surface of the acoustic product. Each acoustic element has front and rear major surfaces extending in the XY plane and side edges extending in the Z direction between the front and rear surfaces. The front surface is the surface that faces a room or other space that will benefit from the sound-absorbing properties.

[0020] Each front face is ground as flat as possible and a further facing is then usually bonded to it. The first and second facings are then at the back of the two acoustic products produced.

[0021] Acoustic products formed by the method of the first aspect of the invention or according to the second and third aspects of the invention may be formed into a suspended ceiling system comprising a plurality of acoustic products suspended in a grid. It is also useful to provide a wall system comprising a plurality of acoustic products as defined by the second or third aspect of the invention suspended on a wall.

[0022] The method of the present invention includes providing an acoustic element, which may be an acoustically insulating element, but more generally is an acoustically absorbing element, and therefore more generally is capable of absorbing sound waves that reach its surface.

[0023] The acoustic element may be formed from any material known for providing acoustic elements, but is preferably formed from MMVF. Although the acoustic element may be made by casting a wet or fluid material (e.g., made from wet-laid mineral fibers), it is preferred to form the acoustic element from air-laid mineral fibers, typically bonded in a matrix by a binder.

[0024] The binder can be any of the binders known for use in bonding MMVF.

[0025] Preferably, the binder is an organic binder, such as a phenol-formaldehyde binder, a urea-formaldehyde binder, a phenol-urea-formaldehyde binder, or a melamine-formaldehyde binder. Conventionally used phenol-formaldehyde or phenol-urea-formaldehyde (PUF)-based resol binders optionally contain a sugar component. For information on these binders that do not contain a sugar component, see, for example, EP0148050 and EP0996653. For information on these binders that contain a sugar component, see, for example, WO2012 / 076462.

[0026] The binder may be a formaldehyde-free binder, such as binder compositions based on polycarboxy polymers and polyols or polyamines, as disclosed in EP-A-583086, EP-A-990727, EP-A-1741726, US-A-5,318,990 and US-A-2007 / 0173588.

[0027] Another group of non-phenol-formaldehyde binders that can be used in MMVF matrices are addition / elimination reaction products of aliphatic and / or aromatic anhydrides with alkanolamines, as disclosed, for example, in WO 99 / 36368, WO 01 / 05725, WO 01 / 96460, WO 02 / 06178, WO 2004 / 007615, and WO 2006 / 061249. These binder compositions are water-soluble and exhibit excellent binding properties in terms of cure speed and cure density. WO 2008 / 023032 discloses a type of urea-modified binder that provides mineral wool products with reduced water absorption.

[0028] Preferably, the binder for the MMVF is a phenol- and formaldehyde-free water-based adhesive composition; and component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (ii) in the form of one or more crosslinkers Includes:

[0029] Further preferred characteristics of the binder are described below in relation to materials used as adhesives, and all of the same preferred characteristics are applicable independently of the adhesive characteristics when this class of material is used as a binder for MMVF in acoustic elements.

[0030] The density of the acoustic element is preferably 40 to 180 kg / m 3 , preferably 80 to 160 kg / m 3 , preferably 100 to 140 kg / m 3 More preferably, it is at least 100 kg / m 3 In particular, in many cases, 150 kg / m 3 It's super.

[0031] When the acoustic element is formed from MMVF, the loss on ignition (LOI) of the man-made vitreous fiber batt bonded by the binder is in the range of 0.5 to 8 wt. %, preferably 2 to 5 wt. LOI is conventionally referred to as binder content. In addition to the primary bonding component, the binder may typically contain small amounts of oil and other organic binder additives.

[0032] When the acoustic element is formed from MMVF, the MMVF generally has an average fiber diameter in the range of 3 to 8 microns.

[0033] The acoustic element is typically in the form of a panel having first and second main faces that are essentially parallel (and extend in the XY direction), connected by a mirrored surface that is typically perpendicular to the main faces (and therefore extends in the Z direction).

[0034] When the acoustic elements are formed from MMVF, they are formed by standard processes for the manufacture of MMVF panels.

[0035] MMV fibers may be made from a mineral melt, which is conventionally provided by providing mineral materials and melting them in a furnace, which may be any of the types of furnace known for producing melt for MMVF, such as a shaft furnace, e.g., a hot metal furnace, a tank furnace, or a cyclone-fired furnace.

[0036] Any suitable method may be used to form MMVF from the melt by fiberization. Fiberization can be by a spinning cup process in which the melt is centrifugally extruded through orifices in the wall of a rotating cup (also known as internal centrifugation, spinning cup). Alternatively, fiberization can be by forcing the melt into a single fiber. This can be by centrifugal fiberization by projecting and spinning them off onto the outer surface of a fiberization rotor or onto a cascade of multiple fiberization rotors rotating around a generally horizontal axis (cascade spinner).

[0037] A binder for the fibers is applied as the fibers are formed and entrained in the air. The fibers may be initially collected on a collector as a primary web, which is then conventionally cross-lapped to form a secondary web.

[0038] The first facing is preferably applied to the first major surface before the step of curing the binder for the MMVF. This is also the case for the second facing, when used. This means that the adhesive for the facing(s) can also be cured in the same curing step as the binder. However, it is also possible to apply the facing(s) after the binder for the matrix of the MMVF has cured, and then carry out the step of curing the adhesive.

[0039] When a second facing is applied, preferably the adhesive for the second facing is of the same chemical type as the adhesive for the first facing.

[0040] Curing of the adhesive is preferably carried out at a temperature of 100 to 300°C, for example 170 to 270°C, for example 180 to 250°C, for example 190 to 230°C.

[0041] In a preferred embodiment, curing of the adhesive is carried out in a conventional curing oven for mineral wool production, preferably operating at a temperature of 150-300°C, such as 170-270°C, for example 180-250°C, for example 190-230°C.

[0042] In one embodiment, the curing is carried out for a time period of 30 seconds to 20 minutes, for example, 1 to 15 minutes, for example, 2 to 10 minutes.

[0043] In a typical embodiment, the curing is carried out at a temperature of 150 to 250° C. for a time of 30 seconds to 20 minutes.

[0044] If the acoustical product is a bonded web of MMVF, the web also contains a binder, which must also be cured. The curing process for the binder may begin immediately after application of the binder to the fibers.

[0045] Curing of an adhesive and / or binder is defined as the process by which the adhesive / binder composition undergoes a physical and / or chemical reaction, which in the case of a chemical reaction typically increases the molecular weight of compounds in the adhesive / binder composition and thereby increases the viscosity of the adhesive / binder composition, typically until the adhesive / binder composition reaches a solid state. The cured binder composition binds the fibers together to form a structurally viscous matrix of fibers. The cured adhesive composition bonds the facing(s) to the acoustic element.

[0046] In one embodiment, the curing of the adhesive / binder is carried out in a heat press. Curing the binder in contact with the mineral fibers in a heat press has the particular advantage of allowing for the production of a high density product.

[0047] In one embodiment, the curing process involves drying by pressure, which may be applied by blowing air or gas through / over the product to be cured.

[0048] The two products may be made by forming a cured fiber batt with first and second facings bonded to first and second major surfaces, respectively, and then cutting the batt into two equal halves parallel to the major surfaces. Each half has a cut surface that will become the front surface of the acoustic product. Each front surface is polished to be as flat as possible.

[0049] In the above method, it is also possible to apply a further facing to the front surface, which is preferably applied using a dry binder rather than an adhesive according to the invention.

[0050] Preferably, the method of the present invention is according to WO2005 / 095727. According to this method, the acoustic product collecting the air-entrained MMVF in a moving collector and, optionally after cross-lapping, vertically compressing the collected fibers to form a web; Reorienting the fibers to provide an unbonded batt having a density of 70 to 200 kg / m3 and increased fiber orientation in the Z direction; curing the binder to form a cured batt; cutting the cured batt in the XY plane into two cutting pads at locations in the Z dimension, wherein the fibers have increased orientation in the Z direction; and, Each cut surface is smoothed by polishing to produce a flat, smooth surface. The film is made by a process including:

[0051] Preferably, first and preferably second facings are applied to the first and second major surfaces of the batt prior to the curing step.

[0052] The above method may also include the conventional step of forming elements having the desired XY dimensions by subdividing the hardened batt and then cutting it into two cut batts, and / or by subdividing the hardened batt before or after grinding to form elements having the desired XY dimensions.

[0053] Cutting of the joined batts can be done conventionally, for example, using a band saw or rotary saw with a suitably small tooth size, similar to a conventional fine wood saw. Sanding or grinding can be with an abrasive belt or any other abrasive or grinding element. The abrasive particles on the belt can be relatively coarse, so that the sanding can be similar to a conventional coarse wood sander or grinder.

[0054] Further details of the preferred method of manufacture can be found in WO2005 / 095727.

[0055] Acoustic products have a thickness, which is the perpendicular distance between the main faces of the product, which is typically in the range of 12 to 100 mm, for example 15 to 50 mm.

[0056] The acoustic products preferably have a length in the range of 550-650 mm or in the range of 1100-1300 mm. Preferred lengths are around 600 mm and around 1200 mm. For special products, the length can be up to 3000 mm, but this may be less preferred due to practical problems with handling and installation.

[0057] Acoustic products have widths ranging from 550 to 650 mm. A preferred width is approximately 600 mm. For special products, lengths as small as 150 mm may be preferred, although this increases installation time, for design reasons or to utilize product parts that would otherwise be discarded.

[0058] The first, second and further facings may independently be any of the materials known for use as facings for acoustical products. Preferably, the or each facing is a fiber veil, particularly a fiberglass veil. The fiberglass veil may itself be bonded by a binder, for example, any of the conventional binders known for bonding matrices of MMVF. The binder content of the veil may range from 10 to 25%, for example, from 12 to 23%.

[0059] An example of such a glass veil is Owens Corning I50U. Another example is Evalith Glass Fiber Veil DH50 / 20. Another suitable glass veil is Saint-Gobain Adfors Glass Veil U 50 D75.

[0060] Facing, e.g., glass fiber veil, 20-80 g / m 2 in the range of 40 to 60 g / m 2 The area weight may be in the range of 1000 to 15000.

[0061] In the above method, adhesive is typically applied to the first facing, and, when used, the second facing, before the facings are brought into contact with the respective major surfaces of the acoustic element. However, it is possible to apply adhesive directly to the major surfaces of the element to which the facings will be adhered.

[0062] The application weight is preferably 5 to 12 g / m 2 , preferably 7 to 10 g / m 2 The applicable weight is in the range of m 2 The dry solid content per unit.

[0063] Preferably, the adhesive is applied by passing the facing through a coating bath containing the adhesive. Another method of application is by spraying.

[0064] Any of the facings may be provided with a paint coating, which may be applied to the facings before or after bonding to the acoustic element.

[0065] The product is an acoustic product and therefore preferably has good sound absorption properties, for example the sound absorption coefficient α is preferably at least 0.7, more preferably at least 0.8, more preferably at least 0.85, even more preferably at least 0.9 or 0.95. The sound absorption coefficient α is determined at the front surface.

[0066] The acoustic products made by the method of the present invention, and the acoustic products of the third aspect of the present invention, may be used in any of the known applications for acoustic products.

[0067] For example, it may be a ceiling tile or forming part of a suspended ceiling, or it may be used as a wall tile or as a baffle. Although acoustic products may be joined directly to a wall or ceiling, it is usually desirable to provide ceiling tiles that are attached to a grid, and in particular suspended from a grid.

[0068] The adhesive used in accordance with the present invention is in the form of an aqueous composition. Preferred features are discussed below. When the acoustic product is formed from MMVF bonded by a binder, the binder may also be of the type discussed below, with all the same preferred features applying.

[0069] The man-made vitreous fiber (MMVF) used in the present invention can be MMVF bonded together by a cured binder, such as glass fiber, ceramic fiber, basalt fiber, slag wool, mineral wool, and stone wool. Bonded MMVF (also described as mineral fibers) are generally produced by conventionally converting a melt of suitable raw materials into fibers, for example, by a spinning cup process or by a cascade rotor process. The fibers are blown into a forming chamber, sprayed while floating and hot with a binder solution, and randomly deposited as a mat or web onto a moving conveyor. The fiber mat is then transferred to a curing oven, where heated air is blown through the mat to cure the binder and firmly bond the mineral fibers together.

[0070] The acoustical products of the present invention utilize a phenol- and formaldehyde-free water-based adhesive (and optionally binder) composition, which comprises: component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (ii) in the form of one or more crosslinkers Includes:

[0071] In particular, the adhesive is a phenol- and formaldehyde-free aqueous composition, component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (ii) in the form of one or more crosslinkers Including, However, the aqueous composition Molecular weight M below 500 W An epoxy compound having The crosslinking agent selected from the group consisting of:

[0072] In particular, the adhesive is a phenol- and formaldehyde-free aqueous composition, component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (ii) in the form of one or more crosslinkers Including, However, the aqueous composition ·Formula R-[C(O)R1] x During the ceremony: R represents a saturated or unsaturated and linear, branched or cyclic hydrocarbon radical, a radical containing one or more aromatic nuclei consisting of 5 or 6 carbon atoms, a radical containing one or more aromatic heterocycles containing 4 or 5 carbon atoms and oxygen, nitrogen or sulfur atoms, the R radicals may contain other functional groups, R1 is a hydrogen atom or a C1-C 10 represents an alkyl radical, x ranges from 1 to 10 a carbonyl compound selected from the aldehydes and carbonyl compounds of The crosslinking agent selected from the group consisting of:

[0073] In particular, the adhesive is a phenol- and formaldehyde-free aqueous composition, - component (i) in the form of one or more lignosulfonate lignins, based on the dry weight of the lignosulfonate lignins, in an amount of 0.03 to 2.0 mmol / g, for example 0. the component having a carboxylic acid group content of 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, - component (ii) in the form of one or more crosslinkers, Including, However, the aqueous composition Polyamines The crosslinking agent selected from the group consisting of:

[0074] In particular, the adhesive is a phenol- and formaldehyde-free aqueous composition, component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (ii) in the form of one or more crosslinkers, Including, However, the aqueous composition Monosaccharides and oligosaccharides The crosslinking agent selected from the group consisting of:

[0075] In one embodiment, the adhesive is a phenol- and formaldehyde-free water-based composition; component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; -below β-hydroxyalkylamide crosslinkers, such as N-(2-hydroxyisopropyl)amide crosslinkers, such as N-(2-hydroxyethyl)amide crosslinkers, such as N-(2-hydroxyethyl)adipamide crosslinkers, such as N,N,N',N'-tetrakis(2-hydroxyethyl)adipamide, and / or polyfunctional organic amines, such as alkanolamines, diamines, such as hexamethyldiamine, and / or epoxy compounds with a molecular weight greater than 500, for example epoxidized oils based on fatty acid triglycerides or one or more flexible oligomers or polymers, for example low-Tg acrylic polymers, for example low-Tg vinyl polymers, for example low-Tg polyethers, containing reactive functional groups such as carbodiimide groups, for example anhydride groups, for example oxazoline groups, for example amino groups, for example epoxy groups, and / or one or more crosslinkers in the form of polyfunctional carbodiimides, for example aliphatic polyfunctional carbodiimides, and / or Primid XL-552, Component (ii) in the form of one or more crosslinkers selected from Including, However, the aqueous composition Molecular weight M below 500 W An epoxy compound having ·Formula R-[C(O)R1] x During the ceremony, R represents a saturated or unsaturated and linear, branched or cyclic hydrocarbon radical, a radical containing one or more aromatic nuclei consisting of 5 or 6 carbon atoms, a radical containing one or more aromatic heterocycles containing 4 or 5 carbon atoms and oxygen, nitrogen or sulfur atoms, the R radicals may contain other functional groups, R1 is a hydrogen atom or a C1-C 10 represents an alkyl radical, x ranges from 1 to 10 a carbonyl compound selected from the aldehydes and carbonyl compounds of the formula: Polyamines The crosslinking agent selected from the group consisting of: Optionally, the aqueous composition comprises: - component (iii) in the form of one or more plasticizers Further includes:

[0076] In one embodiment, the adhesive is a phenol- and formaldehyde-free water-based composition; component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (ii) in the form of one or more crosslinkers, - component (iii) in the form of one or more plasticizers Includes:

[0077] In particular, the adhesive is a phenol- and formaldehyde-free aqueous composition, component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (ii) in the form of one or more crosslinkers, - component (iii) in the form of one or more plasticizers Including, However, the aqueous binder composition Molecular weight M below 500 W An epoxy compound having The crosslinking agent selected from the group consisting of:

[0078] In particular, the adhesive is a phenol- and formaldehyde-free aqueous composition, component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (ii) in the form of one or more crosslinkers, - component (iii) in the form of one or more plasticizers Including, However, the aqueous composition ·Formula R-[C(O)R1] x During the ceremony, R represents a saturated or unsaturated and linear, branched or cyclic hydrocarbon radical, a radical containing one or more aromatic nuclei consisting of 5 or 6 carbon atoms, a radical containing one or more aromatic heterocycles containing 4 or 5 carbon atoms and oxygen, nitrogen or sulfur atoms, the R radicals may contain other functional groups, R1 is a hydrogen atom or a C1-C 10 represents an alkyl radical, x ranges from 1 to 10 a carbonyl compound selected from the aldehydes and carbonyl compounds of The crosslinking agent selected from the group consisting of:

[0079] In particular, the adhesive is a phenol- and formaldehyde-free aqueous composition, component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (ii) in the form of one or more crosslinkers, - component (iii) in the form of one or more plasticizers Including, Polyamines The crosslinking agent selected from the group consisting of:

[0080] In particular, the adhesive is a phenol- and formaldehyde-free aqueous composition, component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (ii) in the form of one or more crosslinkers, - component (iii) in the form of one or more plasticizers Including, However, the aqueous composition Monosaccharides and oligosaccharides The crosslinking agent selected from the group consisting of:

[0081] In one embodiment, the adhesive is a phenol- and formaldehyde-free aqueous composition comprising: component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; -below β-hydroxyalkylamide crosslinkers, and / or epoxy compounds with a molecular weight greater than 500, for example epoxidized oils based on fatty acid triglycerides or one or more flexible oligomers or polymers, for example low-Tg acrylic polymers, for example low-Tg vinyl polymers, for example low-Tg polyethers, containing reactive functional groups such as carbodiimide groups, for example anhydride groups, for example oxazoline groups, for example amino groups, for example epoxy groups, and / or one or more crosslinkers in the form of polyfunctional carbodiimides, for example aliphatic polyfunctional carbodiimides; and / or ·Primid XL-552; Component (ii) in the form of one or more crosslinkers selected from component (iii) in the form of one or more plasticizers, Including, The aqueous composition Molecular weight M below 500 W An epoxy compound having ·Formula R-[C(O)R1] x During the ceremony, R represents a saturated or unsaturated and linear, branched or cyclic hydrocarbon radical, a radical containing one or more aromatic nuclei consisting of 5 or 6 carbon atoms, a radical containing one or more aromatic heterocycles containing 4 or 5 carbon atoms and oxygen, nitrogen or sulfur atoms, and the R radical is It may contain other functional groups, R1 is a hydrogen atom or a C1-C 10 represents an alkyl radical, x ranges from 1 to 10 a carbonyl compound selected from the aldehydes and carbonyl compounds of Polyamines The crosslinking agent selected from the group consisting of:

[0082] In a preferred embodiment, the adhesive is formaldehyde-free.

[0083] For the purposes of this application, the term "formaldehyde-free" means that the formaldehyde emissions from a mineral wool product are 5 μg / m 2 / hour, preferably less than 3 μg / m 2 This is defined to characterize mineral wool products that have an aldehyde emission rate of less than 1 / hour. Preferably, the test is performed according to ISO 16000 for testing aldehyde emissions.

[0084] In a preferred embodiment, the adhesive is phenol-free.

[0085] For purposes of this application, the term "phenol-free" means that the aqueous composition does not contain phenol in an amount of ≦0.25 wt. %, such as ≦0.1 wt. %, for example ≦0.05 wt. %, based on the total weight of the aqueous composition having a dry solids binder content of 15 wt. %.

[0086] [ka]

[0087] is defined to contain

[0088] In one embodiment, the adhesive composition contains no added formaldehyde.

[0089] In one embodiment, the adhesive composition does not contain added phenol.

[0090] For purposes of the present invention, the term "mono- and oligosaccharides" is defined to include mono- and oligosaccharides having 10 or fewer saccharide units.

[0091] For purposes of the present invention, the term "sugar" is defined to include monosaccharides and oligosaccharides having 10 or fewer saccharide units.

[0092] Component (i) Component (i) is in the form of one or more lignosulfonate lignins and has a carboxylic acid group content, based on the dry weight of the lignosulfonate lignin, of 0.03 to 2.0 mmol / g, for example 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g.

[0093] Lignin, cellulose, and hemicellulose are the three main organic compounds in plant cell walls. Lignin can be thought of as a glue, holding the cellulose fibers together. It contains both hydrophilic and hydrophobic groups. Lignin is the second most abundant natural polymer in the world after cellulose, and is estimated to represent 20-30% of the total carbon contained in biomass worldwide, which exceeds 1 billion tons.

[0094] The lignosulfonate process introduces a large number of sulfonate groups that make lignin soluble not only in water but also in acidic aqueous solutions. Lignosulfonates have up to 8% of the sulfur as sulfonates, while kraft lignin has 1-2% of the sulfur, mostly bound to the lignin. The molecular weight of lignosulfonates ranges from 15,000 to 50,000 g / mol. The typical hydrophobic core of lignin, combined with the large number of ionized sulfonate groups, makes this lignin attractive as a surfactant, often finding use in dispersing cement and other materials.

[0095] To produce lignin-based value-added products, lignin must first be separated from biomass, and several methods can be used for this purpose. Kraft and sulfite pulping processes are known for their effective separation of lignin from wood and are therefore used worldwide. Kraft lignin is separated from wood with the aid of NaOH and NaS. Lignin from the sulfite pulping process is designated lignosulfonate and is produced by using sulfite and / or sulfite salts containing magnesium, calcium, sodium, or ammonium at varying pH levels. Currently, lignosulfonates account for 90% of the total commercial lignin market, with a total annual global production of lignosulfonates of approximately 1.8 million tons. Lignosulfonates generally have a large number of sulfonic acid groups and therefore a higher amount of sulfur than kraft lignin. Due to the presence of sulfonated groups, lignosulfonates are anionically charged and water-soluble. The molecular weight (Mw) of lignosulfonates can be comparable to or greater than that of kraft lignin. Due to these unique properties, lignosulfonates have a wide range of uses, for example, as animal feed, pesticides, surfactants, additives in oil drilling, stabilizers in colloidal suspensions, and plasticizers in concrete admixtures. However, because the majority of new pulp mills use kraft technology for pulp production, kraft lignin is more readily available for value-added manufacturing.

[0096] However, lignosulfonates and kraft lignin have different properties and functional group distributions resulting from their different isolation processes. The high level of sulfonic acid groups in lignosulfonates, generally at least one per every four C9 units, makes lignosulfonates highly charged in water at all pH levels. This abundance of ionic functional groups may explain much of the difference compared to other industrial lignins. The higher charge density allows for easier water solubility and a higher solids content in solution compared to kraft lignin. For the same reason, lignosulfonates also have a lower solution viscosity at the same solids content, which may facilitate handling and processing. A commonly used model structure of lignosulfonates is shown in Figure 1.

[0097] In one embodiment, component (i) has a carboxylic acid group content of 0.05 to 0.6 mmol / g, for example 0.1 to 0.4 mmol / g, based on the dry weight of the lignosulfonate lignin.

[0098] In one embodiment, component (i) has an average carboxylic acid group content per polymer, taking into account the weight average M_n of component (i), of less than 1.8 groups, for example less than 1.4 groups, for example less than 1.1 groups, such as less than 0.7 groups, such as less than 0.4 groups.

[0099] In one embodiment, component (i) has a content of phenolic OH groups of 0.3 to 2.5 mmol / g, such as 0.5 to 2.0 mmol / g, for example 0.5 to 1.5 mmol / g, based on the dry weight of the lignosulfonate lignin.

[0100] In one embodiment, component (i) has a content of aliphatic OH groups of 1.0 to 8.0 mmol / g, such as 1.5 to 6.0 mmol / g, for example 2.0 to 5.0 mmol / g, based on the dry weight of the lignosulfonate lignin.

[0101] In one embodiment, component (i) comprises ammonium lignosulfonate and / or calcium lignosulfonate and / or magnesium lignosulfonate, and any combination thereof.

[0102] In one embodiment, component (i) comprises ammonium lignosulfonate and calcium lignosulfonate, and + Against Ca 2+ The molar ratio of these is in the range of 5:1 to 1:5, particularly 3:1 to 1:3.

[0103] For purposes of the present invention, the term "lignosulfonate" includes sulfonated kraft lignin.

[0104] In one embodiment, component (i) is sulfonated kraft lignin.

[0105] In one embodiment, the aqueous composition contains added sugars in an amount of 0 to 5 wt %, for example less than 5 wt %, for example 0 to 4.9 wt %, for example 0.1 to 4.9 wt %, based on the weight of lignosulfonate and sugars.

[0106] In one embodiment, the aqueous composition comprises component (i), i.e., the lignosulfonate, in an amount of 50 to 98 wt.%, such as 65 to 98 wt.%, for example 80 to 98 wt.%, based on the total weight of components (i) and (ii).

[0107] In one embodiment, the aqueous composition comprises component (i) in an amount of 50 to 98 wt. %, for example 65 to 98 wt. %, for example 80 to 98 wt. %, based on the dry weight of components (i), (ii), and (iii).

[0108] For the purposes of the present invention, the content of lignin functional groups is 31 It is determined by using P NMR as a characterization method.

[0109] 31P NMR sample preparation was performed using 2-chloro-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane (TMDP) as the phosphitylation reagent and cholesterol as the internal standard. Integration was from the work of Granata and Argyropoulos (J. Agric. Food Chem. 43:1538-1544).

[0110] Component (ii) Component (ii) is in the form of one or more crosslinkers.

[0111] In one embodiment, component (ii) comprises one or more crosslinkers selected from, in one embodiment, β-hydroxyalkylamide-crosslinkers and / or oxazoline-crosslinkers. .

[0112] β-Hydroxyalkylamide crosslinkers are curing agents for acid-functional polymers. They provide hard, durable, corrosion-resistant, and solvent-resistant crosslinked polymer networks. β-Hydroxyalkylamide crosslinkers are believed to cure through an esterification reaction to form multiple ester linkages. The hydroxy functionality of the β-hydroxyalkylamide crosslinker should average at least 2, preferably greater than 2, and more preferably 2-4, to obtain optimal crosslinking response.

[0113] Oxazoline group-containing crosslinking agent is a polymer containing one or more oxazoline groups in each molecule, and generally, oxazoline-containing crosslinking agent can be easily obtained by polymerizing oxazoline derivatives. Patent US6818699B2 provides a disclosure about such a process.

[0114] In one embodiment, component (ii) is one or more epoxy compounds having a molecular weight greater than 500, for example, an epoxidized oil based on a fatty acid triglyceride or one or more flexible oligomers or polymers, for example, a low Tg acrylic polymer, for example, a low Tg vinyl polymer, for example, a low Tg polyether, containing reactive functional groups such as carbodiimide groups, for example, an anhydride group, for example, an oxazoline group, for example, an amino group, for example, an epoxy group, for example, a β-hydroxyalkylamide group.

[0115] In one embodiment, component (ii) is one or more crosslinkers selected from the group consisting of fatty amines.

[0116] In one embodiment, component (ii) is one or more crosslinkers in the form of a fatty amide.

[0117] In one embodiment, component (ii) is one or more crosslinkers selected from polyester polyols, such as polycaprolactone.

[0118] In one embodiment, component (ii) is one or more cross-linking agents selected from the group consisting of starch, modified starch, CMC.

[0119] In one embodiment, component (ii) is one or more crosslinkers in the form of a polyfunctional carbodiimide, for example an aliphatic polyfunctional carbodiimide.

[0120] In one embodiment, component (ii) is one or more cross-linking agents in the form of an aziridine, for example CX100, NeoAdd-Pax 521 / 523.

[0121] In one embodiment, component (ii) is one or more crosslinkers selected from melamine-based crosslinkers, such as hexakis(methylmethoxy)melamine (HMMM)-based crosslinkers.

[0122] Examples of such compounds are Picassian XL 701, 702, 725 (Stahl polymers), e.g. ZOLDINE® XL-29SE (Angus Chemical Company), e.g. CX300 (DSM), e.g. Carbodilite V-02-L2 (Nisshinbo Chemical Inc.).

[0123] In one embodiment, component (ii) is Primid XL552, which has the following structure:

[0124] [ka]

[0125] Component (ii) may also be a mixture of any of the above compounds.

[0126] In one embodiment, the adhesive composition comprises component (ii) in an amount of 1 to 50 wt %, such as 4 to 20 wt %, for example 6 to 12 wt %, based on the dry weight of component (i).

[0127] In one embodiment, component (ii) is β-hydroxyalkylamide crosslinkers, such as N-(2-hydroxyisopropyl)amide crosslinkers, such as N-(2-hydroxyethyl)amide crosslinkers, such as N-(2-hydroxyethyl)adipamide crosslinkers, such as N,N,N',N'-tetrakis(2-hydroxyethyl)adipamide, and / or polyfunctional organic amines, such as alkanolamines, diamines, such as hexamethyldiamine, and / or epoxy compounds with a molecular weight greater than 500, for example epoxidized oils based on fatty acid triglycerides or one or more flexible oligomers or polymers, for example low Tg acrylic polymers, for example low Tg vinyl polymers, for example low Tg polyethers, containing reactive functional groups such as carbodiimide groups, for example anhydride groups, for example oxazoline groups, for example amino groups, for example epoxy groups; and / or one or more crosslinkers in the form of polyfunctional carbodiimides, for example aliphatic polyfunctional carbodiimides and one or more cross-linking agents selected from:

[0128] In one embodiment, component (ii) is β-Hydroxyalkylamide crosslinkers, such as N-(2-hydroxyisopropyl)amide crosslinkers, such as N-(2-hydroxyethyl)amide crosslinkers, such as N-(2-hydroxyethyl)adipamide crosslinkers, such as N,N,N',N'-tetrakis(2-hydroxyethyl)adipamide The compound includes one or more cross-linking agents selected from the group consisting of:

[0129] In one embodiment, component (ii) comprises component (ii) in an amount of 2 to 90% by weight, such as 6 to 60% by weight, for example 10 to 40% by weight, for example 25 to 40% by weight, based on the dry weight of component (i).

[0130] Component (iii) of the adhesive composition The adhesive composition may include component (iii), which is in the form of one or more plasticizers.

[0131] In one embodiment, component (iii) is a polyol, such as a carbohydrate, a hydrogenated sugar, such as sorbitol, erythritol, glycerol, monoethylene glycol, polyethylene glycol, polyethylene glycol ether, polyether, phthalate, and / or an acid, such as adipic acid, vanillic acid, lactic acid and / or ferulic acid, acrylic acid, The polymer may be in the form of one or more plasticizers selected from the group consisting of polymers, polyvinyl alcohol, polyurethane dispersions, ethylene carbonate, propylene carbonate, lactones, lactams, lactides, acrylic polymers with free carboxy groups and / or polyurethane dispersions with free carboxy groups, polyamides, amides such as carbamide / urea, or any mixture thereof.

[0132] In one embodiment, component (iii) is in the form of one or more plasticizers selected from the group consisting of carbonates, e.g., ethylene carbonate, propylene carbonate, lactones, lactams, lactides, compounds having a structure similar to lignin, such as vanillin, acetosyringone, alcohol ethers, solvents used as coalescents, such as polyvinyl alcohol.

[0133] In one embodiment, component (iii) is in the form of one or more non-reactive plasticizers selected from the group consisting of polyethylene glycols, polyethylene glycol ethers, polyethers, hydrogenated sugars, phthalates and / or other esters, alcohol ethers, acrylic polymers, solvents used as coalescents such as polyvinyl alcohol.

[0134] In one embodiment, component (iii) is one or more reactive plasticizers selected from the group consisting of carbonates, such as ethylene carbonate, propylene carbonate, lactones, lactams, lactides, di- or tricarboxylic acids, such as adipic acid or lactic acid, and / or vanillic acid and / or ferulic acid, polyurethane dispersions, acrylic polymers with free carboxy groups, vanillin, compounds with a structure similar to lignin, such as acetosyringone.

[0135] In one embodiment, component (iii) is in the form of one or more plasticizers selected from the group consisting of fatty alcohols, monohydroxy alcohols, such as pentanol, stearyl alcohol.

[0136] In one embodiment, component (iii) comprises one or more plasticizers selected from the group consisting of polyethylene glycol, polyethylene glycol ethers, and / or one or more plasticizers in the form of a polyol, for example 1,1,1-tris(hydroxymethyl)propane, and / or triethanolamine.

[0137] Another particularly surprising aspect of the adhesive compositions used in the present invention is that the use of plasticizers with boiling points above 100°C, in particular between 140 and 250°C, strongly improves the mechanical properties of the acoustic products of the present invention, although in view of these boiling points it is likely that these plasticizers may at least partially evaporate in contact with the mineral fibers during curing of the adhesive.

[0138] In one embodiment, component (iii) comprises one or more plasticizers having a boiling point above 100°C, for example, from 110 to 380°C, more preferably from 120 to 300°C, more preferably from 140 to 250°C.

[0139] The effectiveness of these plasticizers in adhesive compositions is believed to be related to their effect of increasing the mobility of lignin during the cross-linking process, which is believed to facilitate effective cross-linking.

[0140] In one embodiment, component (iii) comprises one or more polyethylene glycols having an average molecular weight of 150 to 50,000 g / mol, in particular 150 to 4,000 g / mol, more particularly 150 to 1,000 g / mol, preferably 150 to 500 g / mol, more preferably 200 to 400 g / mol.

[0141] In one embodiment, component (iii) comprises one or more polyethylene glycols having an average molecular weight of 4000 to 25000 g / mol, in particular 4000 to 15000 g / mol, more particularly 8000 to 12000 g / mol.

[0142] In one embodiment, component (iii) is capable of forming a covalent bond with component (i) and / or component (ii) during the curing process. Such a component does not evaporate and remain as part of the composition, but is effectively modified so as not to cause undesirable side effects, such as water absorption, in the cured product. Non-limiting examples of such components include caprolactone and acrylic polymers with free carboxyl groups.

[0143] In one embodiment, component (iii) is selected from the group consisting of fatty alcohols, monohydroxy alcohols such as pentanol, stearyl alcohol.

[0144] In one embodiment, component (iii) is selected from one or more plasticizers selected from the group consisting of alkoxylates, for example, ethoxylates, for example, butanol ethoxylates, for example, butoxytriglycol.

[0145] In one embodiment, component (iii) is selected from one or more propylene glycols.

[0146] In one embodiment, component (iii) is selected from one or more glycol esters.

[0147] In one embodiment, component (iii) is selected from one or more plasticizers selected from the group consisting of phenol derivatives, for example, alkyl or aryl substituted phenols.

[0148] In one embodiment, component (iii) is selected from one or more plasticizers selected from the group consisting of silanols, siloxanes.

[0149] In one embodiment, component (iii) is one or more plasticizers selected from the group consisting of sulfates, e.g., alkyl sulfates, sulfonates, e.g., alkylaryl sulfonates, e.g., alkyl sulfonates, phosphates, e.g., tripolyphosphates; e.g., tributyl phosphate.

[0150] In one embodiment, component (iii) is selected from one or more hydroxy acids.

[0151] In one embodiment, component (iii) is selected from one or more plasticizers selected from the group consisting of monomeric amides, such as acetamide, benzamide, fatty acid amides, such as tall oil amide.

[0152] In one embodiment, component (iii) is selected from one or more plasticizers selected from the group consisting of quaternary ammonium compounds, for example, trimethylglycine, distearyldimethylammonium chloride.

[0153] In one embodiment, component (iii) is selected from one or more plasticizers selected from the group consisting of vegetable oils, such as castor oil, palm oil, linseed oil, tall oil, soybean oil.

[0154] In one embodiment, component (iii) is in the form of tall oil.

[0155] In one embodiment, component (iii) is selected from one or more plasticizers selected from the group consisting of hydrogenated oils, acetylated oils.

[0156] In one embodiment, component (iii) is selected from one or more fatty acid methyl esters.

[0157] In one embodiment, component (iii) is selected from one or more plasticizers selected from the group consisting of alkyl polyglucosides, gluconamides, amino glucose amides, sucrose esters, sorbitan esters.

[0158] In one embodiment, component (iii) is selected from the group consisting of polyethylene glycol, polyethylene glycol ether.

[0159] In one embodiment, component (iii) is selected from the group consisting of triethanolamine.

[0160] In one embodiment, component (iii) is one or more plasticizers in the form of propylene glycol, phenol derivatives, silanols, siloxanes, hydroxy acids, vegetable oils, polyethylene glycol, polyethylene glycol ethers, and / or polyols, e.g., 1,1,1-tris(hydroxymethyl)propane, triethanolamine, or any mixture thereof.

[0161] It has been found that the inclusion of a plasticizer in the adhesive composition can improve the mechanical properties of the acoustic product of the present invention.

[0162] The term "plasticizer" refers to a substance added to a material to make it softer, more flexible (by decreasing the glass transition temperature, Tg), and easier to process.

[0163] Component (iii) can be a mixture of any of the above compounds.

[0164] In one embodiment, component (iii) is present in an amount of 0.5 to 60, preferably 2.5 to 25, more preferably 3 to 15 wt %, based on the dry weight of component (i).

[0165] In one embodiment, component (iii) is present in an amount of 0.5 to 60, preferably 2.5 to 25, more preferably 3 to 15 wt. %, based on the dry weight of components (i), (ii), and (iii).

[0166] The adhesive resulting from curing the adhesive composition comprises components (i) and (iia), and in one embodiment the adhesive composition comprises: component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of 0.03 to 2.0 mmol / g, such as 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin; - component (iia) in the form of one or more modifiers Including, Preferably, the aqueous adhesive composition Molecular weight M below 500 W and the crosslinking agent is selected from the group consisting of epoxy compounds having the formula: and / or The aqueous adhesive composition ·Formula R-[C(O)R1] x During the ceremony: R represents a saturated or unsaturated and linear, branched or cyclic hydrocarbon radical, a radical containing one or more aromatic nuclei consisting of 5 or 6 carbon atoms, a radical containing one or more aromatic heterocycles containing 4 or 5 carbon atoms and oxygen, nitrogen or sulfur atoms, the R radicals may contain other functional groups, R1 is a hydrogen atom or a C1-C 10 represents an alkyl radical, x ranges from 1 to 10 a carbonyl compound selected from the aldehydes and carbonyl compounds of and does not contain a crosslinking agent selected from and / or The aqueous adhesive composition Polyamines, and does not contain a crosslinking agent selected from and / or The aqueous adhesive composition Monosaccharides and oligosaccharides The crosslinking agent selected from the group consisting of:

[0167] The inventors have found that excellent adhesive properties may also be achieved by a two-component system comprising component (i) in the form of one or more lignosulfonate lignins having a carboxylic acid group content of 0.03 to 2.0 mmol / g, for example 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin, and component (iia) in the form of one or more modifiers, and optionally any of the other components described above and below.

[0168] In one embodiment, component (iia) is a modifying agent in the form of one or more compounds selected from epoxy compounds having a molecular weight greater than 500, for example epoxidized oils based on fatty acid triglycerides or one or more flexible oligomers or polymers, for example low Tg acrylic polymers, for example low Tg vinyl polymers, for example low Tg polyethers, containing reactive functional groups such as carbodiimide groups, for example anhydride groups, for example oxazoline groups, for example amino groups, for example epoxy groups, for example β-hydroxyalkylamide groups.

[0169] In one embodiment, component (iia) is one or more modifying agents selected from the group consisting of polyethyleneimine, polyvinylamine, fatty amine.

[0170] In one embodiment, component (iia) is one or more modifying agents selected from polyfunctional carbodiimides, such as aliphatic polyfunctional carbodiimides.

[0171] Component (iia) may be a mixture of any of the compounds listed above.

[0172] Without wishing to be bound by any particular theory, the inventors attribute the excellent adhesive properties achieved by adhesive compositions comprising components (i) and (iia) and optional further components to the effect that the modifier used as component (iia) at least partially performs the functions of a plasticizer and a crosslinker.

[0173] In one embodiment, the adhesive composition comprises component (iia) in an amount of 1 to 40 wt %, such as 4 to 20 wt %, for example 6 to 12 wt %, based on the dry weight of component (i).

[0174] Further ingredients In some embodiments, the adhesive comprises additional components.

[0175] In one embodiment, the adhesive composition comprises a catalyst selected from inorganic acids such as sulfuric acid, sulfamic acid, nitric acid, boric acid, hypophosphorous acid, and / or phosphoric acid, and / or any salts thereof, such as sodium hypophosphite, and / or ammonium salts such as ammonium salts of sulfuric acid, sulfamic acid, nitric acid, boric acid, hypophosphorous acid, and / or phosphoric acid, and / or sodium polyphosphate (STTP) and / or sodium metaphosphate (STMP), and / or phosphorus oxychloride. The presence of such a catalyst may improve the curing properties of the adhesive composition.

[0176] In one embodiment, the adhesive composition comprises a Lewis acid, such as ZnCl, Mg(ClO), Sn[N(SO-n-CF], or the like, which can accept an electron pair from a donor compound to form a Lewis adduct. 17 )2]4.

[0177] In one embodiment, the adhesive composition comprises a catalyst selected from metal chlorides such as KCl, MgCl, ZnCl, FeCl, and SnCl or adducts thereof such as AlCl adducts, BF adducts, such as BF ethylamine complex.

[0178] In one embodiment, the adhesive composition includes a catalyst selected from organometallic compounds, such as titanate-based catalysts and tin-based catalysts.

[0179] In one embodiment, the adhesive composition comprises a catalyst selected from chelating agents, such as transition metals, e.g., iron ions, chromium ions, manganese ions, copper ions, and / or peroxides, e.g., organic peroxides, e.g., dicumyl peroxide.

[0180] In one embodiment, the adhesive composition according to the present invention comprises a catalyst selected from a phosphite, such as an alkyl phosphite, such as an aryl phosphite, such as triphenyl phosphite.

[0181] In one embodiment, the adhesive composition according to the present invention comprises a catalyst selected from the group consisting of tertiary amines, for example, tris-2,4,6-dimethylaminomethylphenol.

[0182] In one embodiment, the adhesive composition further comprises an additional component (iv) in the form of one or more silanes.

[0183] In one embodiment, the adhesive composition further comprises one or more coupling agents, for example component (iv), in the form of an organofunctional silane.

[0184] In one embodiment, component (iv) is selected from the group consisting of organofunctional silanes, such as primary or secondary amino-functionalized silanes, epoxy-functionalized silanes, such as polymeric or oligomeric epoxy-functionalized silanes, methacrylate-functionalized silanes, alkyl- and aryl-functionalized silanes, urea-functionalized silanes, or vinyl-functionalized silanes.

[0185] In one embodiment, the adhesive composition further comprises component (v) in the form of one or more components selected from the group consisting of a base, such as ammonia, such as an alkali metal hydroxide, such as KOH, such as an alkaline earth metal hydroxide, such as Ca(OH)2, such as Mg(OH)2, such as an amine, or any salt thereof.

[0186] In one embodiment, the adhesive composition further comprises a further component in the form of urea, especially in an amount of 5 to 40% by weight, for example 10 to 30% by weight, 15 to 25% by weight, based on the dry weight of component (i).

[0187] In one embodiment, the adhesive composition comprises a further component in the form of one or more carbohydrates selected from the group consisting of sucrose, reducing sugars, in particular dextrose, polycarbohydrates and mixtures thereof, preferably dextrins and maltodextrins, more preferably glucose syrup, more preferably glucose syrup having a dextrose equivalent value of DE=30-100 or less, such as DE=60-100 or less, for example DE=60-99, such as DE=85-99, for example DE=95-99.

[0188] In one embodiment, the adhesive composition comprises a further component in the form of one or more carbohydrates selected from the group consisting of sucrose and reducing sugars in an amount of 5 to 50% by weight, such as 5 to less than 50% by weight, for example 10 to 40% by weight, for example 15 to 30% by weight, based on the dry weight of component (i).

[0189] In one embodiment, the adhesive composition comprises an additional component in the form of one or more silicone resins.

[0190] In one embodiment, the adhesive composition according to the invention comprises a further component (vi) in the form of one or more reactive or non-reactive silicones.

[0191] In one embodiment, component (vi) is selected from the group consisting of silicones composed of a backbone composed of organosiloxane residues, in particular diphenylsiloxane residues, alkylsiloxane residues, preferably dimethylsiloxane residues, bearing at least one hydroxyl, carboxyl or anhydride, amine, epoxy or vinyl functional group capable of reacting with at least one of the components of the adhesive composition, and is preferably present in an amount of 0.025 to 15 wt. %, preferably 0.1 to 10 wt. %, more preferably 0.3 to 8 wt. %, based on adhesive solids.

[0192] In one embodiment, the adhesive composition includes an additional component in the form of one or more mineral oils.

[0193] In the context of the present invention, adhesive compositions having a sugar content of 50% or more by weight, based on the total dry weight of the adhesive components, are considered to be sugar-based adhesives. In the context of the present invention, adhesive compositions having a sugar content of less than 50% by weight, based on the total dry weight of the adhesive components, are considered to be non-sugar-based adhesives.

[0194] In one embodiment, the adhesive composition comprises further components in the form of one or more surfactants, such as non-ionic and / or ionic emulsifiers, e.g., polyoxyethylene (4) lauryl ether, e.g., soybean lecithin, e.g., sodium dodecyl sulfate.

[0195] The use of lignin-based sulfonated products in adhesives may result in an increase in the hydrophilicity of some adhesives and final products, which means that one or more hydrophobic agents are added, such as one or more mineral oils, one or more silicone oils, one or more silicone resins.

[0196] In one embodiment, the aqueous adhesive composition component (i) in the form of one or more lignins selected from the following group: 0.03-2.0mmol / based on the dry weight of lignosulfonate lignin g, for example 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g; and / or - component (ii) in the form of one or more crosslinkers, component (iii) in the form of one or more plasticizers, - one or more coupling agents, for example component (iv) in the form of organofunctional silanes, optionally a component in the form of one or more compounds selected from the group consisting of a base, such as ammonia, an alkali metal hydroxide, such as KOH, an alkaline earth metal hydroxide, such as Ca(OH) 2, such as Mg(OH) 2, an amine or any salt thereof, - optionally a component in the form of urea, - optionally a component in the form of a more reactive or non-reactive silicone, optionally a hydrocarbon oil, optionally one or more surfactants, -water It essentially consists of:

[0197] In one embodiment, the aqueous adhesive composition component (i) in the form of one or more lignins selected from the following group: Lignosulfonate lignin having a carboxylic acid group content of 0.03 to 2.0 mmol / g, for example 0.03 to 1.4 mmol / g, for example 0.075 to 2.0 mmol / g, for example 0.075 to 1.4 mmol / g, based on the dry weight of the lignosulfonate lignin. and / or - component (ii) in the form of one or more crosslinkers, - one or more coupling agents, for example component (iv) in the form of organofunctional silanes, optionally a component in the form of one or more compounds selected from the group consisting of a base, such as ammonia, an alkali metal hydroxide, such as KOH, an alkaline earth metal hydroxide, such as Ca(OH) 2, such as Mg(OH) 2, an amine or any salt thereof, - optionally a component in the form of urea, - optionally a component in the form of a more reactive or non-reactive silicone, optionally a hydrocarbon oil, optionally one or more surfactants, -water It essentially consists of:

[0198] The inventors have surprisingly found that mineral fiber products (such as the acoustic product of the present invention) comprising the aqueous adhesive composition described above have very high stability both when freshly produced and after aging conditions when the aqueous adhesive composition is used as a binder in the mineral fiber product.

[0199] Additionally, the inventors have found that even greater product stability can be obtained by using cure temperatures >230°C.

[0200] The inventors have further found that the stability of the product can be further increased by the following means. -Low line capacity means longer cure time -Silicone resin addition -Adding a large amount of crosslinking agent - Addition of a combination of two or more different crosslinkers - Addition of small amounts of cationic species, such as polyvalent metal ions, e.g. calcium, and / or organic cationic species, e.g. amines and / or organically modified inorganic compounds, e.g. amine-modified montmorillonite clay.

[0201] When the acoustic product comprises mineral fibers, such fibers may be any man-made vitreous fiber (MMVF), such as glass fiber, ceramic fiber, basalt fiber, slag fiber, rock fiber, stone fiber, etc. These fibers may be present, for example, as wool products, such as stone wool products.

[0202] Fiber / melt composition The man-made vitreous fibers (MMVF) may have any suitable oxide composition. The fibers may be glass fibers, ceramic fibers, basalt fibers, slag fibers, or rock or stone fibers. The fibers are preferably of the type commonly known as rock, stone, or slag fibers, and most preferably are stone fibers.

[0203] Stone fibers generally contain the following oxides in weight percent: SiO2: 30-51 Al2O3: 12-30 CaO: 8-30 MgO: 2 to 25 FeO (including Fe2O3): 2-15 Na2O+K2O: 10 or less CaO+MgO: 10-30

[0204] In a preferred embodiment, the MMVF has the following levels of elements, calculated as oxides in wt %: SiO2: at least 30, 32, 35 or 37; not more than 51, 48, 45 or 43 Al2O3: at least 12, 16, or 17; not more than 30, 27, or 25 CaO: at least 8 or 10; not more than 30, 25 or 20 MgO: at least 2 or 5; not more than 25, 20 or 15 FeO (including Fe2O3): at least 4 or 5; not more than 15, 12, or 10 FeO+MgO: at least 10, 12, or 15; not more than 30, 25, or 20 Na2O+K2O: zero or at least 1; 10 or less CaO+MgO: at least 10 or 15; not more than 30 or 25 TiO2: zero or at least 1; up to 6, 4, or 2 TiO2 + FeO: at least 4 or 6; not more than 18 or 12 B2O3: zero or at least 1; 5 or less than 3 P2O5: zero or at least 1; 8 or less than 5 Other: zero or at least one; eight or five or less

[0205] The MMVF used in the present invention preferably has the following composition in weight percent: SiO235~50 Al2O312~30 TiO2 max 2 Fe2O33~12 CaO 5-30 MgO max 15 Na2O 0~15 K2O 0~15 P2O5 max 3 MnO max 3 B2O3 max 3

[0206] Another preferred composition for MMVF is as follows in weight percent: SiO2 39-55%, preferably 39-52% Al2O3 16-27%, preferably 16-26% CaO 6-20%, preferably 8-18% MgO 1 to 5%, preferably 1 to 4.9% Na2O 0-15%, preferably 2-12% K2O 0-15%, preferably 2-12% R2O (Na2O + K2O) 10 to 14.7%, preferably 10 to 13.5% P2O50-3%, preferably 0-2% Fe2O3 (total iron) 3-15%, preferably 3.2-8% B2O3 0-2%, preferably 0-1% TiO2 0-2%, preferably 0.4-1% Other 0~2.0%

[0207] Glass fibers generally contain the following oxides, in weight percent: SiO2: 50-70 Al2O3: 10-30 CaO: 27 or less MgO: 12 or less

[0208] The glass fibers may also contain the following oxides, in weight percent: Na2O+K2O: 8-18, especially Na2O+K2O more than CaO+MgO B2O3:3~12

[0209] Some glass fiber compositions may contain less than 2% Al2O3. [Brief explanation of the drawings]

[0210] [Figure 1] Figure 1 shows a commonly used model structure of a lignosulfonate. [Figure 2] FIG. 2 is a perspective view of an acoustic product according to the present invention. [Figure 3] FIG. 3 is a schematic diagram of the method of the present invention up to the curing oven stage. [Figure 4] FIG. 4 is a schematic of the configuration of FIG. 6 after the curing oven. DETAILED DESCRIPTION OF THE INVENTION

[0211] The acoustic product 1 of Figure 2 has a smooth, flat, sound-absorbing front surface 2, a rear surface 3, and side edges 4 extending in the Z direction between the front and rear surfaces, which extend in what is called the XY plane. The acoustic product also consists of acoustic elements on the front surface 2 and rear surface 3, which are bonded MMVF matrices with facings. The side edges 4 may be square or have some other shape.

[0212] As shown in Figure 3, a typical apparatus for making the product includes a cascade spinner 6 having multiple front-mounted rotors 7 positioned to receive melt from a melt gutter 8, such that the melt falls onto the rotors and is dumped as fibers from one rotor to the next. Air entrains these fibers at and near the rotors 7, carrying them into a collection chamber 9 having a perforated collector conveyor 10 at its base. Air is drawn through the collector, forming a web 11 on the collector and transporting it out of the collection chamber 9 onto another conveyor 12. The primary web 11 is guided by conveyor 12 into the top of cross-lapping pendulum 13, which causes layers of the primary web to cross-lap against each other as they are collected as secondary web 15A below the pendulum in conveyor 14.

[0213] Secondary web 15A is guided by conveyor 14 to a pair of conveyors 16 which apply vertical compression to the secondary web from its natural depth at point A to its compressed depth at point B. The secondary web at point A has a weight per unit area of ​​W.

[0214] The compressed secondary web 15B is transferred from point C to point D by conveyor 17. Conveyors 16 and 17 typically all move at substantially the same speed to establish a constant rate of travel of the secondary web from vertical compression stage AB to point D.

[0215] The web is then transported between a pair of conveyors 18 extending between points E and F. Conveyors 18 move significantly slower than conveyors 16 and 17 so that longitudinal compression is applied between points D and F.

[0216] Although items 14, 16, 17 and 18 are shown for clarity as conveyor belts spaced apart in the X direction, in reality they will typically be very close to each other in the X direction.

[0217] Points D and E are preferably sufficiently close to one another or interconnected by a band to prevent the secondary web from deviating from the desired line of travel. As a result, substantial longitudinal compression occurs when the web emerges at point F. A restraining guide can be provided between D and E, if necessary, to prevent web breakage when D and E are not close together.

[0218] The resulting longitudinally compressed batt 15C is then conveyed by conveyor 18 at a higher speed along conveyor 19 between points G and H. This applies some longitudinal decompression or expansion to the longitudinally compressed web to prevent the web from slipping out of the desired line of travel and from collapsing inward due to internal forces within the web, for example. If desired or necessary, a conveyor or other guide (not shown) may be on the top surface of the batt (above conveyor 19) to ensure slippage is not possible.

[0219] When vertical compression is to be applied to the longitudinally compressed web, this is done by passing the web after leaving point H between conveyors and conveyor 20 which converge to compress the web vertically as it travels between points I and J.

[0220] The resulting uncured batt 15D has first and second major surfaces 3A and 3B. A fiberglass veil 22 from roll 23 then contacts surfaces 3A and 3B. The glass veil 22 is applied with an adhesive, as needed by the present invention, to bond the veil to the batt. The resulting assembly then passes through curing oven 25, where just enough pressure is applied by conveyor 24 to hold the two-layer sandwich of veil 22 and batt 15D together while the curing of the binder and adhesive for the MMVF occurs.

[0221] The spliced ​​batt 15E emerges from the curing oven and is sliced ​​down the center by a bandsaw 26 or other suitable saw into two cut batts 27, each having an outer surface 3 carrying the bale 22 and an inner cutting surface 2 (see FIG. 4). Each cut batt 27 is supported on a conveyor 28 and moves down an abrasive belt 29 where it is polished or ground to a flat configuration and additional facings 22 are applied from rolls 30 and bonded to the polished surface 2. The polished or ground cut batt 27 is then cut by a suitable cutter 31. , divided into individual vats 1 which are carried away by a conveyor 32.

[0222] The paint may be applied to either or both sides.

[0223] Although conveyor bands or belts are shown throughout this specification, any or all of the conveyors may be replaced by any suitable means for causing relative transport by acceleration, deceleration, or vertical compression when required. For example, a roller train may be used instead of a belt.

[0224] Adhesive example In the following examples, several adhesives falling within the definition of adhesives used in the present invention were prepared and compared with prior art adhesives.

[0225] The following properties were determined for the adhesive used in the present invention and for the prior art adhesive, respectively:

[0226] Adhesive component solid content The content of each component in a given adhesive solution before curing is based on the anhydrous weight of the component.

[0227] Lignosulfonates were supplied as liquids with approximately 50% solids content by Borregaard, Norway, and LignoTech, Florida. Primid XL552 was supplied by EMS-CHEMIE AG, Silane (Momentive VS-142, 40% active) and calculated as 100% for simplicity. Silicone resin BS1052 was supplied by Wacker Chemie AG. NH4OH (24.7%) was supplied by Univar and used in the form supplied. PEG200, urea, KOH pellets, and 1,1,1 tris(hydroxymethyl)propane were supplied by Sigma-Aldrich and assumed to be anhydrous for simplicity.

[0228] adhesive solid The adhesive content after curing is referred to as "adhesive solids."

[0229] Disk-shaped stone wool samples (diameter: 5 cm; height: 1 cm) were cut from the stone wool and heat-treated at 580°C for at least 30 minutes to remove all organic matter. The solids of the adhesive mixture were measured by distributing a sample of the adhesive mixture (approximately 2 g) onto the heat-treated stone wool disc in a tin foil container. The weight of the tin foil container containing the stone wool disc was weighed before and immediately after adding the adhesive mixture. Two such stone wool discs were prepared by placing them in a tin foil container and heating them at 200°C for 1 hour. After cooling and storing at room temperature for 10 minutes, the samples were weighed, and the adhesive solids were calculated as the average of the two results. An adhesive with the desired adhesive solids could then be prepared by diluting with the required amount of water and 10% aqueous silane (Momentive VS-142).

[0230] mechanical strength research Bar Exam The mechanical strength of the adhesive (when tested as a binder for the MMVF matrix) was tested in a bar test: for each binder, 16 bars were produced from a mixture of the binder and stone wool shot from a stone wool spinning production.

[0231] A sample of this binder solution with a dry solids content of 15% (16.0 g) was thoroughly mixed with shot (80.0 g). The resulting mixture was then filled into four slots of a heat-resistant silicone form to make small bars (4 x 5 slots per form; slot top dimensions: length = 5.6 cm, width = 2.5 cm; slot bottom dimensions: length = 5.3 cm, width = 2.2 cm; slot height = 1.1 cm). The slotted mixture was then pressed with a suitably sized flat metal bar to create a uniform bar surface. 16 bars from each binder were produced in this manner. The resulting bars were then cured, typically at 225°C. The curing time was 1 hour. After cooling to room temperature, the bars were carefully removed from the container. Five of the bars were aged in a water bath at 80°C for 3 hours. This method of curing the prepared bars was used, for example, in Tables 1.1, 1.2, 1.4, 1.5, and 1.6. The results in Table 1.3 are based on a slightly different method, including a preconditioning step at 90°C for 2 hours, followed by curing at 225°C for 1 hour, while the rest of the procedure is the same.

[0232] After drying for 3 days, the aged bars as well as the five unaged bars were subjected to a three-point bending test on a Bent Tram machine (test speed: 10.0 mm / min; fracture level: 50%; apparent strength: 30 N / mm 2 Support distance: 40mm; Maximum deflection: 20mm; Apparent elastic modulus: 10000N / mm 2 ) and their mechanical strength was investigated. The bars were placed in the machine with the "top" side up (i.e. the side with dimensions length=5.6 cm, width=2.5 cm).

[0233] Adhesive example, reference adhesive (phenol-formaldehyde resin modified with urea and PUF-resol) The adhesive is a phenol-formaldehyde resin modified with urea, a PUF-resol.

[0234] A phenol-formaldehyde resin is prepared by reacting 37% aqueous formaldehyde (606 g) and phenol (189 g) in the presence of 46% aqueous potassium hydroxide (25.5 g) at 84°C, after first heating at a rate of approximately 1°C per minute. The reaction is continued at 84°C until the resin has an acid resistance of 4 and most of the phenol has been converted. Urea (241 g) is then added and the mixture is cooled.

[0235] Acid resistance (AT) represents the number of times a given volume of adhesive can be diluted with acid without the mixture becoming cloudy (the adhesive settling). Sulfuric acid is used to determine the stopping criteria in adhesive production, with an acid resistance of less than 4 indicating the end of the adhesive reaction.

[0236] To measure the AT, a titrant is prepared by diluting 2.5 ml of concentrated sulfuric acid (>99%) with 1 L of deionized water. 5 ml of the adhesive under investigation is then titrated with this titrant at room temperature by manually shaking the adhesive; if preferred, using a magnetic stirrer and magnetic stick; while keeping the adhesive in motion. Titration is continued until a slight cloudiness appears in the adhesive that does not disappear when the adhesive is shaken.

[0237] Acid resistance (AT) is calculated by dividing the amount of acid (in mL) used in the titration by the amount of sample (in mL). AT = (titration volume used (mL)) / (sample volume (mL))

[0238] Using the resulting urea-modified phenol-formaldehyde resin, an adhesive is made by adding 25% aqueous ammonia (90 mL) and ammonium sulfate (13.2 g), followed by water (1.30 kg).

[0239] The adhesive solids were then measured as above and the mixture was diluted with the amount of water and silane required for the mechanical measurement (15% adhesive solids solution, 0.5% silane of adhesive solids).

[0240] Adhesive example, reference adhesive (alkali-oxidized lignin-based adhesive) 3267 kg of water was charged into a 6000 L reactor, followed by 287 kg of aqueous ammonia (24.7%). Then, 1531 kg of lignin, UPM BioPiva 100 was added slowly over a period of 30 to 45 minutes. The mixture was heated to 40°C and held at this temperature for 1 hour. After 1 hour, a check was made for insolubilized lignin. This can be done by checking the solution on a glass plate or Hegman gauge. Insolubilized lignin is visible as small particles in the brown adhesive. During the dissolution step, the lignin solution changes color from brown to glossy black. After the lignin is completely dissolved, 1 liter of foam wetting agent (Skumdaemper 11-10 from NCÅ-Verodan) is added. The batch temperature is maintained at 40°C. Then, the addition of 307.5 kg of 35% hydrogen peroxide is started. The hydrogen peroxide is dosed at a rate of 200 to 300 L / hour. The first half of the hydrogen peroxide is added at a rate of 200 L / hour, after which the dosing rate is increased to 300 L / hour.

[0241] During the addition of hydrogen peroxide, the temperature in the reaction mixture is controlled by heating or cooling to reach a final reaction temperature of 65°C.

[0242] The final product was analyzed for COOH content, dry solids, pH, viscosity, and residual H2O2. 60 g of this oxidized lignin (18.2% solids) was mixed with 1.4 g of Primid XL552 (100% solids) and 2.8 g of PEG200 (100% solids). 0.6 g of Silane (Momentive VS-142, 40% active, 10% in water) and 17.4 g of water were added and mixed to obtain 15% solids, which was then used for mechanical property testing in a bar test.

[0243] Adhesive Compositions for Use in the Present Invention In the following, the entry numbers of the adhesive examples correspond to the entry numbers used in Tables 1-1 to 1-6.

[0244] The carboxylic acid group content of all lignosulfonates used in the adhesive according to the invention is 31 As measured using P NMR, it was found to be in the range of 0.05–0.6 mmol / g based on the dry weight of lignosulfonate lignin in all cases.

[0245] Example 2 To 30.0 g of the lignosulfonate solution (50% solids), 0.4 g of NH4OH (24.7%) was added and mixed, followed by 1.9 g of Primid XL552 (100% solids) and mixed in. Finally, 0.7 g of Silane (Momentive VS-142, 40% active, 10% in water) and 64.3 g of water were added and mixed to give 15% solids, which was then used for mechanical property testing in a bar test.

[0246] Example 11 To 30.0 g of the lignosulfonate solution (50% solids), 0.4 g of NH4OH (24.7%) was added and mixed, followed by 2.1 g of Primid XL552 (100% solids) and 3.4 g of PEG200 (100% solids). Finally, 0.7 g of Silane (Momentive VS-142, 40% active, 10% in water) and 61.8 g of water were added and mixed to give 15% solids, which was then used for mechanical property testing in a bar test.

[0247] Example 15 To 30.0 g of the lignosulfonate solution (50% solids), 0.4 g of NH4OH (24.7%) was added and mixed, followed by 2.9 g of Primid XL552 (100% solids) and 3.4 g of PEG200 (100% solids). Finally, 0.8 g of Silane (Momentive VS-142, 40% active, 10% in water) and 67 g of water were added and mixed to give 15% solids, which was then used for mechanical property testing in a bar test.

[0248] Example 30 To 30.0 g of the lignosulfonate solution (50% solids), 0.4 g of NH4OH (24.7%) was added and mixed, followed by 2.9 g of Primid XL552 (100% solids) and 3.4 g of 1,1,1 tris(hydroxymethyl)propane (100% solids). Finally, 0.8 g of Silane (Momentive VS-142, 40% active, 10% in water) and 67 g of water were added and mixed to give 15% solids, which was then used for mechanical property testing in bar tests.

[0249] Example 33 To 100.0 g of the lignosulfonate solution (50% solids), 0.3 g of KOH was added in pellet form and mixed, followed by 10.8 g of Primid XL552 (100% solids) and 11.3 g of PEG200 (100% solids) and mixed in. Finally, 2.6 g of Silane (Momentive VS-142, 40% active, 10% in water) and 228 g of water were added and mixed to give 15% solids, which was then used for mechanical property testing in a bar test.

[0250] Example 41 To 30.0 g of the lignosulfonate solution (50% solids), 0.4 g of NH4OH (24.7%) was added and mixed, followed by 1.9 g of Primid XL552 (100% solids), 1.7 g of PEG200 (100% solids), and 1.7 g of urea (100% solids). Finally, 0.7 g of Silane (Momentive VS-142, 40% active, 10% in water) and 60.5 g of water were added and mixed to give a 15% solids content, which was then used for mechanical property testing in a bar test.

[0251] The mechanical properties are shown in Tables 1.1 to 1.6. For simplicity, the amounts of all other components are recalculated based on 100 g of dry lignin.

[0252] As can be seen from Table 1.1, a combination of crosslinker (Primid XL 552) and plasticizer (PEG200) is required to achieve high mechanical properties (unaged and aged strength in bar test) at levels comparable to the reference adhesive (11 and 15 vs. 2 and 9 vs. reference adhesive).

[0253] Tables 1.2 and 1.3 show that different plasticizers can be used (13 and 15 vs. 30) or the combination of plasticizer (34 vs. 41) and PEG200 is the preferred plasticizer.

[0254] Table 1.4 shows that the addition of silane can help achieve the same level of aged strength as the reference adhesive.

[0255] Table 1.5 shows that adhesives have high strength without the presence of a base, but with a non-permanent base (NH4O This shows that adding PEG-100 (H) or a permanent base (KOH) to the formulation can protect manufacturing equipment from corrosion without significantly altering strength.

[0256] Table 1.6 shows that different lignosulfonates can be used.

[0257] Overall, this means that we are able to produce mineral wool products based on phenol- and formaldehyde-free adhesive compositions with a high content of lignin-based renewable materials that have mechanical properties comparable to reference systems and can be produced in a simpler and less expensive way.

[0258] [Table 1]

[0259] [Table 2]

[0260] [Table 3]

[0261] [Table 4]

[0262] [Table 5]

[0263] [Table 6]

[0264] Examples 47 to 50 In the following, the entry numbers of the adhesive examples correspond to the entry numbers used in Table 2.

[0265] The carboxylic acid group content of all lignosulfonates used in the adhesive according to the invention is 31 P NMR was used to determine the range of 0.05-0.6 mmol / g based on the dry weight of lignosulfonate lignin, but for this particular batch used in Examples 47, 48, 49, 50, 51, 52, 53, and 54, it was found to be 0.1 It was found to be 4 mmol / g.

[0266] Example 47 To 30.0 g of the lignosulfonate solution (50% solids), 0.4 g of NH4OH (24.7%) was added and mixed, followed by 0.7 g of Silane (Momentive VS-142, 40% active, 10% in water) and 68.9 g of water and mixing to give 15% solids, which was then used for testing mechanical properties in a bar test.

[0267] Example 49 To 30.0 g of the lignosulfonate solution (50% solids), 0.4 g of NH4OH (24.7%) was added and mixed, followed by 6.0 g of Primid XL552 (100% solids) and mixed in. Finally, 1.0 g of Silane (Momentive VS-142, 40% active, 10% in water) and 102.6 g of water were added and mixed to give 15% solids, which was then used for mechanical property testing in a bar test.

[0268] The mechanical properties are shown in Table 2. For simplicity, the amounts of all other components are recalculated based on 100 g of dry lignin.

[0269] As can be seen from Table 2, for the combination of lignosulfonate and cross-linking agent (Primid XL 552), the higher the amount of cross-linking agent, the better the mechanical properties.

[0270] [Table 7] [Example]

[0271] Example I - Peel Strength Fleece (Johns Manville glass fiber nonwoven Everlith DH 50 / 20) was cut into 3 cm wide strands. Adhesive was applied to the fleece by a roller at a loading level of 40 g / m². The fleece with adhesive was pressed onto a finished MMVF product with a density of 145 kg / m³ at a pressure of 2500 Pa and cured at 200-225°C for 45 minutes. The binder in the MMVF product was prepared as follows:

[0272] 730.0 kg of ammonium lignosulfonate was placed in a stirred vessel, to which 8.5 L of NH4OH (24.7%) was added and stirred. 151 kg of Primid XL552 solution (pre-made 31 wt% solution in water) and 43 kg of PEG200 (100% solids) were then added and mixed, followed by 13 kg of Silane (Momentive VS-142, 40% active, 10% in water) and 40 kg of silicone (Wacker BS 1052, 12% in water). The curing oven temperature was set to 275°C.

[0273] After the adhesive cured, the product was allowed to cool at room temperature for 2 hours and the bond strength was measured by pulling the edge of the fleece strand with a Mecmesin force gauge in a pulling direction perpendicular to the surface of the MMVF product. The bond strength is expressed in grams.

[0274] This method was carried out with four different adhesives to bond the fleece to the MMVF product.

[0275] Adhesive 1 according to the present invention was prepared as follows. To 200.0 g of the lignosulfonate solution (50% solids), 2.5 g of NH4OH (24.7%) was added and mixed, followed by 20.0 g of Primid XL552 (100% solids) and 23.0 g of PEG200 (100% solids) and mixed in. Finally, 120.3 g of water was added and mixed to give 35% solids, which was then used to test adhesion.

[0276] Comparative Adhesive 1 is made as follows (PUF adhesive). A phenol-formaldehyde resin is prepared by reacting 37% aqueous formaldehyde (606 g) and phenol (189 g) in the presence of 46% aqueous potassium hydroxide (25.5 g) at 84°C, after first heating at a rate of approximately 1°C per minute. The reaction is continued at 84°C until the resin has an acid resistance of 4 and most of the phenol has been converted. Urea (241 g) is then added and the mixture is cooled.

[0277] Acid resistance (AT) represents the number of times a given volume of adhesive can be diluted with acid without the mixture becoming cloudy (the adhesive settling). Sulfuric acid is used to determine the stopping criteria in adhesive production, with an acid resistance of less than 4 indicating the end of the adhesive reaction.

[0278] To measure the AT, a titrant is prepared by diluting 2.5 ml of concentrated sulfuric acid (>99%) with 1 L of deionized water. 5 ml of the adhesive under investigation is then titrated with this titrant at room temperature by manually shaking the adhesive; if preferred, using a magnetic stirrer and magnetic stick; while keeping the adhesive in motion. Titration is continued until a slight cloudiness appears in the adhesive that does not disappear when the adhesive is shaken.

[0279] Acid resistance (AT) is calculated by dividing the amount of acid (in mL) used in the titration by the amount of sample (in mL). AT = (titration volume used (mL)) / (sample volume (mL))

[0280] Using the resulting urea-modified phenol-formaldehyde resin, an adhesive is made by adding 25% aqueous ammonia (90 mL) and ammonium sulfate (13.2 g), followed by water (1.30 kg).

[0281] The adhesive solids were then measured as above and the mixture diluted with the required amount of water and silane (15% adhesive solids solution, 0.5% silane of adhesive solids).

[0282] Comparative Adhesive 2 (lignin-based adhesive) is prepared as follows. 3267 kg of water was charged into a 6000 L reactor, followed by 287 kg of aqueous ammonia (24.7%). Then, 1531 kg of lignin, UPM BioPiva 100 was added slowly over a period of 30 to 45 minutes. The mixture was heated to 40°C and held at this temperature for 1 hour. After 1 hour, a check was made for insolubilized lignin. This can be done by checking the solution on a glass plate or Hegman gauge. Insolubilized lignin is seen as small particles in the brown adhesive. During the dissolution step, the lignin solution changes color from brown to shiny black. After complete dissolution, add 1 liter of foam wetting agent (Skumdaemper 11-10 from NCÅ-Verodan). Maintain the batch temperature at 40°C. Then begin adding 307.5 kg of 35% hydrogen peroxide. The hydrogen peroxide is dosed at a rate of 200-300 L / hour. The first half of the hydrogen peroxide is added at a rate of 200 L / hour, after which the dose rate is increased to 300 L / hour.

[0283] During the addition of hydrogen peroxide, the temperature in the reaction mixture is controlled by heating or cooling to reach a final reaction temperature of 65°C.

[0284] The final product was analyzed for COOH content, dry solids, pH, viscosity, and residual H2O2. 60 g of this oxidized lignin (18.2% solids) was mixed with 1.4 g of Primid XL552 (100% solids) and 2.8 g of PEG200 (100% solids). 0.6 g of Silane (Momentive VS-142, 40% active, 10% in water) and 17.4 g of water were added and mixed to obtain 15% solids.

[0285] Comparative Adhesive 3 is made as follows (formaldehyde-free, sugar-based adhesive).

[0286] A mixture of 75.1% aqueous glucose syrup (19.98 g; so effectively 15.0 g glucose syrup), 50% aqueous hypophosphorous acid (0.60 g; so effectively 0.30 g, 4.55 mmol hypophosphorous acid) and sulfamic acid (0.45 g, 4.63 mmol) in water (30.0 g) was stirred at room temperature until a clear solution was obtained.

[0287] 28% aqueous ammonia (0.80 g; so effectively 0.22 g, 13.15 mmol of ammonia) was then added dropwise until pH = 7.9. The adhesive solids were then determined (21.2%).

[0288] The binder mixture was diluted with water (0.403 g / g binder mixture) and 10% aqueous silane (0.011 g / g binder mixture, Momentive VS-142). The final binder mixture for mechanical strength studies had a pH of 7.9.

[0289] The results are shown in Table I. As can be seen from Table I, when the adhesive of the present invention is used to bond a fleece to an MMVF product, the peel strength is slightly lower than PUF, but is improved compared to the comparative formaldehyde-free binder.

[0290] [Table 8]

Claims

1. 1. A method of manufacturing an acoustic product, comprising: providing an acoustic element including first and second major surfaces; providing a first facing; securing the first facing to a first major surface of the acoustic element with an adhesive; and curing the adhesive wherein the adhesive is a phenol- and formaldehyde-free aqueous adhesive composition; and Component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of from 0.03 to 2.0 mmol / g, for example from 0.03 to 1.4 mmol / g, for example from 0.075 to 2.0 mmol / g, for example from 0.075 to 1.4 mmol / g, based on the dry weight of said lignosulfonate lignin; Component (ii) in the form of one or more crosslinkers Including, Component (i) is in the form of one or more lignosulfonate lignins having an average carboxylic acid group content per polymer, taking into account the M_n weight average of component (i), of less than 1.4 groups; The method.

2. The method of claim 1 , wherein the acoustic element is a man-made vitreous fiber (MMVF) panel.

3. the man-made vitreous fiber panel is formed from man-made vitreous fibers bonded together by a cured binder, the binder before curing being a phenol- and formaldehyde-free composition; and Component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of from 0.03 to 2.0 mmol / g, for example from 0.03 to 1.4 mmol / g, for example from 0.075 to 2.0 mmol / g, for example from 0.075 to 1.4 mmol / g, based on the dry weight of said lignosulfonate lignin; Component (ii) in the form of one or more crosslinkers The method of claim 2 , comprising:

4. The method of any one of claims 1 to 3, wherein the first facing is a fiberglass veil.

5. 5. The method of claim 1, wherein the first facing has two major surfaces, the method comprising applying an adhesive to a major surface of the first facing, and then applying the major surface of the first facing to a first major surface of the acoustic element.

6. The method of claim 5 including applying the adhesive with a roller.

7. The method according to any of the preceding claims, wherein the step of curing the adhesive is carried out at a temperature of 100 to 300°C, preferably 170 to 270°C, preferably 180 to 250°C, preferably 190 to 230°C.

8. The acoustic element has a resistance of 40 to 180 kg / m ３ , for example, 80 to 160 kg / m ３ , preferably 100 to 140 kg / m ３ The method according to any one of claims 1 to 7, having a density in the range of Law.

9. The method according to any of the preceding claims, wherein the loss on ignition (LOI) of the acoustic element is in the range of 2 to 8 wt%, preferably 3 to 5 wt%.

10. The method of any preceding claim, including the step of securing a second facing to the second major surface of the acoustic element.

11. 11. The method of claim 10, comprising cutting the cured element in a plane substantially parallel to the major surface, and polishing each cut surface smooth to form two acoustic products.

12. A method according to any preceding claim, wherein the acoustic product has a thickness in the range 12 to 100 mm, for example 15 to 50 mm.

13. A method according to any preceding claim, wherein the acoustic product has a width in the range 550-650 mm, preferably around 600 mm.

14. A method according to any preceding claim, wherein the acoustic product has a length in the range 550 to 650 mm or 1100 to 1300 mm, preferably around 600 mm, preferably around 1200 mm.

15. The adhesive is applied in a dry state at a rate of 5 to 12 g / m ２ The method of any one of claims 1 to 14, comprising applying in an amount of

16. The method according to any one of claims 1 to 15, wherein the acoustic product is a ceiling panel.

17. The method according to any one of claims 1 to 15, wherein the acoustic product is a wall panel.

18. The method according to any one of claims 1 to 15, wherein the acoustic product is a baffle.

19. Acoustic product obtainable by the method according to any one of claims 1 to 18.

20. 1. An acoustic product comprising an acoustic element including first and second major surfaces and a first facing, said first facing secured to said first major surface of said acoustic element by an adhesive, said adhesive composition being phenol- and formaldehyde-free; Component (i) in the form of one or more lignosulfonate lignins, said component having a carboxylic acid group content of from 0.03 to 2.0 mmol / g, for example from 0.03 to 1.4 mmol / g, for example from 0.075 to 2.0 mmol / g, for example from 0.075 to 1.4 mmol / g, based on the dry weight of said lignosulfonate lignin; Component (ii) in the form of one or more crosslinkers Including, Component (i) is in the form of one or more lignosulfonate lignins having an average carboxylic acid group content per polymer, taking into account the M_n weight average of component (i), of less than 1.4 groups; The acoustic product.

21. 21. A suspended ceiling system comprising a plurality of acoustic products according to claim 19 or 20 suspended in a grid.

22. 21. A wall system comprising a plurality of acoustic products according to claim 19 or 20 suspended on a wall.

23. 23. The method, acoustic product or system of any preceding claim, wherein the aqueous adhesive composition further comprises component (iii) in the form of one or more plasticizers.

24. 24. The method, acoustic product or system of any preceding claim, wherein component (i) has a carboxylic acid group content of 0.05 to 0.6 mmol / g, based on the dry weight of the lignosulfonate lignin.

25. 25. The method, acoustic product or system of any preceding claim, wherein component (i) is in the form of one or more lignosulfonate lignins having an average carboxylic acid group content per polymer, taking into account the weight average M_n of component (i), of less than 1.1 groups, such as less than 0.7 groups, for example less than 0.4 groups.

26. 26. The method, acoustic product or system of any preceding claim, wherein component (i) has a content of phenolic OH groups of 0.3 to 2.5 mmol / g, for example 0.5 to 2.0 mmol / g, for example 0.5 to 1.5 mmol / g, based on the dry weight of the lignosulfonate lignin.

27. 27. The method, acoustic product or system of any preceding claim, wherein component (i) has a content of aliphatic OH groups of 1.0 to 8.0 mmol / g, for example 1.5 to 6.0 mmol / g, for example 2.0 to 5.0 mmol / g, based on the dry weight of the lignosulfonate lignin.

28. 28. The method, acoustic product or system of any preceding claim, wherein component (i) comprises ammonium lignosulfonate and / or calcium lignosulfonate and / or magnesium lignosulfonate, and any combination thereof.

29. Component (i) comprises ammonium lignosulfonate and calcium lignosulfonate, and NH ４ ＋ Against Ca ２＋ 29. The method, acoustic product or system according to any one of claims 1 to 28, wherein the molar ratio of is in the range of 5:1 to 1:5, in particular 3:1 to 1:

3.

30. 30. The method, acoustic product, or system of any of claims 1 to 29, wherein the aqueous adhesive composition contains added sugars in an amount of 0 to less than 5% by weight, based on the weight of lignosulfonate and sugars.

31. 31. The method, acoustic product or system of any preceding claim, wherein the aqueous adhesive composition comprises component (i) in an amount of 50 to 98 wt. %, for example 65 to 98 wt. %, for example 80 to 98 wt. %, based on the dry weight of components (i) and (ii).

32. The component (ii) a. β-hydroxyalkylamide-crosslinking agent, and / or b. oxazoline-crosslinking agents, and / or c. polyfunctional organic amines, such as alkanolamines, diamines, such as hexamethyldiamine, and / or d. epoxy compounds having a molecular weight greater than 500, for example, epoxidized oils based on fatty acid triglycerides or one or more flexible oligomers or polymers, for example, low Tg acrylic polymers, for example, low Tg vinyl polymers, for example, low Tg polyethers, containing reactive functional groups such as carbodiimide groups, for example, anhydride groups, for example, oxazoline groups, for example, amino groups, for example, epoxy groups; and / or e. one or more cross-linking agents selected from the group consisting of fatty amines, and / or f. another cross-linking agent in the form of a fatty amide, and / or g. one or more crosslinkers selected from polyester polyols, e.g., polycaprolactone; and / or h. one or more cross-linking agents selected from the group consisting of starch, modified starch, and CMC; and / or i. one or more crosslinkers in the form of a polyfunctional carbodiimide, e.g., an aliphatic polyfunctional carbodiimide, and / or j. one or more crosslinking agents selected from melamine-based crosslinking agents, for example, hexakis(methylmethoxy)melamine (HMMM)-based crosslinking agents 32. The method, acoustic product or system of any preceding claim, in the form of one or more cross-linking agents selected from:

33. 33. The method, acoustic product or system of any preceding claim, wherein component (ii) comprises one or more crosslinkers selected from β-hydroxyalkylamide-crosslinkers and / or oxazoline-crosslinkers.

34. 34. The method, acoustic product or system of any preceding claim, wherein the binder composition comprises component (ii) in an amount of 1 to 50% by weight, for example 4 to 20% by weight, for example 6 to 12% by weight, based on the dry weight of component (i).

35. The component (ii) a. β-hydroxyalkylamide-crosslinkers, such as N-(2-hydroxyisopropyl)amide-crosslinkers, such as N-(2-hydroxyethyl)amide-crosslinkers, such as N-(2-hydroxyethyl)adipamide-crosslinkers, such as N,N,N',N'-tetrakis(2-hydroxyethyl)adipamide, and / or b. Polyfunctional organic amines, such as alkanolamines, diamines, such as hexamethyldiamine, and / or c. Epoxidized oils based on epoxy compounds having a molecular weight greater than 500, for example, fatty acid triglycerides or one or more flexible oligomers or polymers, for example, low Tg acrylic polymers, for example, low Tg vinyl polymers, for example, low Tg polyethers, containing reactive functional groups such as carbodiimide groups, for example, anhydride groups, for example, oxazoline groups, for example, amino groups, for example, epoxy groups, and / or d. one or more crosslinkers in the form of polyfunctional carbodiimides, e.g., aliphatic polyfunctional carbodiimides 35. The method, acoustic product or system of any preceding claim, in the form of one or more cross-linking agents selected from:

36. The component (ii) a. β-hydroxyalkylamide-crosslinkers, such as N-(2-hydroxyisopropyl)amide-crosslinkers, such as N-(2-hydroxyethyl)amide-crosslinkers, such as N-(2-hydroxyethyl)adipamide-crosslinkers, such as N,N,N',N'-tetrakis(2-hydroxyethyl)adipamide 36. The method, acoustic product or system of any preceding claim, comprising one or more cross-linking agents selected from:

37. 37. The method, acoustic product or system of any preceding claim, wherein the adhesive composition comprises component (ii) in an amount of 2 to 90 wt.%, such as 6 to 60 wt.%, for example 10 to 40 wt.%, for example 25 to 40 wt.%, based on the dry weight of component (i).

38. Component (iii) one or more plasticizers selected from the group consisting of fatty alcohols, monohydroxy alcohols, such as pentanol, stearyl alcohol, and / or one or more plasticizers selected from the group consisting of alkoxylates, e.g., ethoxylates, e.g., butanol ethoxylates, e.g., butoxytriglycol, and / or one or more plasticizers in the form of propylene glycol, and / or one or more plasticizers in the form of glycol esters, and / or one or more plasticizers selected from the group consisting of adipate, acetate, benzoate, cyclobenzoate, citrate, stearate, sorbate, sebacate, azelate, butyrate, valerate, and / or one or more plasticizers selected from the group consisting of phenol derivatives, e.g., alkyl- or aryl-substituted phenols, and / or one or more plasticizers selected from the group consisting of silanols, siloxanes, and / or one or more plasticizers selected from the group consisting of sulfates, e.g., alkyl sulfates; sulfonates, e.g., alkylaryl sulfonates, e.g., alkyl sulfonates; phosphates, e.g., tripolyphosphates; and / or one or more plasticizers in the form of hydroxy acids, and / or one or more plasticizers selected from the group consisting of monomeric amides, e.g., acetamide, benzamide, fatty acid amides, e.g., tall oil amide, and / or one or more plasticizers selected from the group consisting of quaternary ammonium compounds, e.g., trimethylglycine, distearyldimethylammonium chloride, and / or one or more plasticizers selected from the group consisting of vegetable oils, such as castor oil, palm oil, linseed oil, soybean oil, and / or tall oil, and / or one or more plasticizers selected from the group consisting of hydrogenated oils, acetylated oils, and / or one or more plasticizers selected from the group consisting of methyl esters of hydroxybenzoates, and / or one or more plasticizers selected from the group consisting of alkyl polyglucosides, gluconamides, amino glucose amides, sucrose esters, sorbitan esters, and / or one or more plasticizers selected from the group consisting of polyethylene glycol, polyethylene glycol ether, and / or one or more plasticizers in the form of a polyol, e.g., glycerol, e.g., 1,1,1-tris(hydroxymethyl)propane, and / or Triethanolamine 38. The method, acoustic product or system of any one of claims 23 to 37, in the form of:

39. 39. The method, acoustic product or system of any one of claims 23 to 38, wherein component (iii) is in the form of propylene glycol, a phenol derivative, a silanol, a siloxane, a hydroxy acid, a vegetable oil, polyethylene glycol, a polyethylene glycol ether, triethanolamine, or any mixture thereof.

40. 40. The method, acoustic product or system of any one of claims 23 to 39, wherein component (iii) comprises one or more plasticizers having a boiling point of from 100 to 380°C, more preferably from 120 to 300°C, more preferably from 140 to 250°C.

41. 41. The method, acoustic product or system according to any one of claims 23 to 40, wherein component (iii) comprises one or more polyethylene glycols having an average molecular weight of 150 to 50,000 g / mol, in particular 150 to 4,000 g / mol, more particularly 150 to 1,000 g / mol, preferably 150 to 500 g / mol, more preferably 200 to 400 g / mol.

42. 42. The method, acoustic product or system of any one of claims 23 to 41, wherein component (iii) is present in the binder composition in an amount of 0.5 to 60, preferably 2.5 to 25, more preferably 3 to 15 wt.%, based on the dry weight of component (i).

43. 43. The method, acoustic product or system of any preceding claim, wherein the adhesive composition further comprises one or more coupling agents, for example component (iv) in the form of an organofunctional silane.

44. The adhesive composition may be prepared by adding a base such as ammonia, an alkali metal hydroxide such as KOH, an alkaline earth metal hydroxide such as Ca(OH) ２ , for example Mg(OH) ２ 44. The method, acoustic product or system of any preceding claim, further comprising component (v) in the form of one or more moieties selected from the group consisting of: an amine or a salt of any of these.

45. 45. The method, acoustic product or system according to any preceding claim, wherein the adhesive composition comprises a further component in the form of urea, in particular in an amount of 5 to 40% by weight, for example 10 to 30% by weight, for example 15 to 25% by weight, based on the dry weight of component (i).

46. 46. ​​A method, acoustic product or system according to any preceding claim, wherein the acoustic element further comprises a further component (vi) in the form of one or more reactive or non-reactive silicones.

47. 47. The method, acoustic product or system of any preceding claim, wherein the acoustic element does not contain ammonia-oxidized lignin (AOL).

48. The aqueous composition Formula R-[C(O)R] １ ] ｘ i. During the ceremony, ii. R represents a saturated or unsaturated and linear, branched or cyclic hydrocarbon radical, a radical containing one or more aromatic nuclei consisting of 5 or 6 carbon atoms, a radical containing one or more aromatic heterocycles containing 4 or 5 carbon atoms and oxygen, nitrogen or sulfur atoms, said R radicals may contain other functional groups; iii. R １ is a hydrogen atom or C １ -C １０ represents an alkyl radical, iv. x ranges from 1 to 10 a carbonyl compound selected from the aldehydes and carbonyl compounds of 48. The method, acoustic product or system of any preceding claim, wherein the method, acoustic product or system is free of a cross-linking agent selected from the group consisting of:

49. 49. The method, acoustic product or system of any preceding claim, wherein the aqueous composition does not comprise a cross-linking agent selected from polyamines.

50. The aqueous composition Molecular weight M of 500 or less Ｗ An epoxy compound having 50. The method, acoustic product or system of any preceding claim, wherein the method, acoustic product or system is free of a cross-linking agent selected from the group consisting of:

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